Water → 3-(4-(4-Methylpiperazin-1-yl)phenyl)butanamide

HRID 1896282노트

반응식

HRID 1896282 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([CH:14]([CH3:18])[CH2:15][C:16]#[N:17])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1.[OH2:19]>C(=O)(O)[O-].[Na+]>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([CH:14]([CH3:18])[CH2:15][C:16]([NH2:17])=[O:19])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1

참가 물질

4

반응물 2

HCID 962WaterHCID 673833103-(4-(4-Methylpiperazin-1-yl)phenyl)butanenitrile

생성물 1

HCID 673827633-(4-(4-Methylpiperazin-1-yl)phenyl)butanamide수율 74%

시약·촉매·용매 1

HCID 516892Sodium Bicarbonate용매

반응 조건

온도
90 °C

실험 절차

A suspension of 3-(4-(4-methylpiperazin-1-yl)phenyl)butanenitrile (450 mg, 1.85 mmol) and poly phosphoric acid (4.5 g) was heated at 90° C. for 3 h. The reaction mixture was cooled to room temperature, diluted with cold water and basified with saturated sodium bicarbonate solution. The aqueous layer was extracted with DCM, washed with water and brine solution. The organic layer was dried over sodium sulfate, filtered and concentrated in vacuo to afford 360 mg (74%) of 3-(4-(4-methylpiperazin-1-yl)phenyl)butanamide as light yellow color solid.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionThe aqueous layer was extracted with DCM
  3. washwashed with water and brine solution
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-8a4e5ab7cc10455bad64765bfc3a8286
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518948B2

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